JPS63168518A - Method for forming platinum black film - Google Patents
Method for forming platinum black filmInfo
- Publication number
- JPS63168518A JPS63168518A JP61312751A JP31275186A JPS63168518A JP S63168518 A JPS63168518 A JP S63168518A JP 61312751 A JP61312751 A JP 61312751A JP 31275186 A JP31275186 A JP 31275186A JP S63168518 A JPS63168518 A JP S63168518A
- Authority
- JP
- Japan
- Prior art keywords
- film
- electrode
- platinum
- voltage
- electrodes
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000012528 membrane Substances 0.000 claims abstract description 15
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000008151 electrolyte solution Substances 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 2
- 229910021607 Silver chloride Inorganic materials 0.000 claims 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims 1
- 229910052697 platinum Inorganic materials 0.000 abstract description 25
- 239000003792 electrolyte Substances 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 4
- UCHOFYCGAZVYGZ-UHFFFAOYSA-N gold lead Chemical compound [Au].[Pb] UCHOFYCGAZVYGZ-UHFFFAOYSA-N 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 238000012544 monitoring process Methods 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 abstract 1
- 229910012463 LiTaO3 Inorganic materials 0.000 abstract 1
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229940046892 lead acetate Drugs 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 229910003781 PbTiO3 Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（イ）産業上の利用分野
この発明は、白金黒膜形成方法に関する。さらに詳しく
は、赤外線の検出や温度検出に有用な各種熱センサにお
ける熱吸収部への熱吸収膜としての白金黒膜の形成方法
に関する。DETAILED DESCRIPTION OF THE INVENTION (a) Field of Industrial Application This invention relates to a method for forming a platinum black film. More specifically, the present invention relates to a method for forming a platinum black film as a heat absorbing film on a heat absorbing portion of various thermal sensors useful for infrared detection and temperature detection.
（ロ）従来の技術
従来、入射赤外線の熱エネルギによる温度上昇とそれに
基づく焦電効果による表面電荷の変化を検知する焦電素
子が、赤外線センサ、感温センサ等の熱センサとして知
られている。かかる焦電素子は、焦電体上に一対の膜状
電極（ＰｔやＡＵ蒸Ｉｉ膜）を形成してその一方（表面
電極）を熱吸収面として構成したものであり、この焦電
体としては、Ｓ ｒ １．＜ Ｂ ａ ｚ Ｎ ｂｚ
Ｏｓ系、Ｐｂ ｓ Ｇｅ ３０ｊＩ系、ＴＧＳ系、Ｐｂ
ＴｔＯ３系、ＰｂＴｉえＺｒ、−エ０３系、Ｌ！ＴａＯ
３系等のセラミックスとＰＶＤＦ等の有機膜が広く用い
られている。そして、検知感度を上昇させるために、熱
吸収面となる一方の膜状電極上に、金黒蒸着膜やカーボ
ンペースト塗布膜を被着する試みがなされている。(B) Conventional technology Conventionally, pyroelectric elements, which detect temperature increases caused by the thermal energy of incident infrared rays and changes in surface charge due to the pyroelectric effect, have been known as thermal sensors such as infrared sensors and temperature sensors. . Such a pyroelectric element is constructed by forming a pair of film-like electrodes (Pt or AU vaporized Ii film) on a pyroelectric body, with one of them (the surface electrode) serving as a heat absorption surface. is S r 1. < B az N bz
Os series, Pb s Ge 30jI series, TGS series, Pb
TtO3 series, PbTiE Zr, -E03 series, L! TaO
Ceramics such as 3-based ceramics and organic films such as PVDF are widely used. In order to increase the detection sensitivity, attempts have been made to deposit a gold black vapor deposited film or a carbon paste coated film on one of the film electrodes, which serves as the heat absorption surface.
そして、この点に関し、本発明者らは、先に、電解によ
り膜状電極上に直接被着形成させた白金黒膜が、熱吸収
性を著しく向上させる事実を見出した。Regarding this point, the present inventors have previously discovered the fact that a platinum black film directly deposited on a membrane electrode by electrolysis significantly improves heat absorption.
〈ハ）発明が解決しようとする問題点
しかしながら、上記無電体のごとき熱変換母材の両面に
膜状電極が形成された熱変換素子を電解液中に浸漬して
その膜状電極の一方（表面電極側）に電解電圧を印加す
ることにより、一方の膜状電極上のみに白金黒膜を形成
させる通常の電解法においては、熱変換母材が比較的薄
い場合に、この母材層を介して他方の膜状電極（裏側電
極）にも電圧が印加されて白金黒がこの裏側電極上にも
回り込んで形成される場合がしばしば生じる。そのため
、電極面積が一定せず約２倍相当になる場合も生じ、電
解条件の調整が困難であり、かつ表面電極上に形成され
る白金黒膜の表面状態も一定せず熱センサとしての感度
に悪影響が生じる問題点があった。<C) Problems to be Solved by the Invention However, it is possible to immerse a heat conversion element in which membrane electrodes are formed on both sides of a heat conversion base material such as the above-mentioned non-electric body in an electrolytic solution, and then immerse one of the membrane electrodes ( In the normal electrolytic method in which a black platinum film is formed only on one membrane electrode by applying an electrolytic voltage to the surface electrode (on the surface electrode side), when the heat conversion base material is relatively thin, this base material layer is A voltage is also applied to the other membrane electrode (back side electrode) through the electrode, and platinum black often wraps around and is formed on this back side electrode. As a result, the electrode area is not constant and may double in some cases, making it difficult to adjust the electrolytic conditions, and the surface condition of the platinum black film formed on the surface electrode is also inconsistent, resulting in poor sensitivity as a thermal sensor. There was a problem with the negative impact on the
この発明は、かかる状況に鑑みなされたものであり、こ
とに上記のごとき両面に電極を備えた素子の一方の電極
面上に電解により選択的に均一な白金黒膜を形成する方
法を提供しようとするものである。The present invention has been made in view of this situation, and particularly provides a method for selectively forming a uniform black platinum film by electrolysis on one electrode surface of an element having electrodes on both sides as described above. That is.
〈二）問題点を解決するための手段
かくしてこの発明によれば、熱変換母材上に一対の膜状
電極を形成した熱変換素子を電解液中に浸漬しその膜状
電極の一方に電解電圧を印加して白金黒膜を電解被着す
ることからなり、電解中に電解被着を意図しない他方の
膜状電極に電解電圧の逆電圧を印加することを特徴とす
る白金黒膜の形成方法が提供される。(2) Means for Solving the Problems Thus, according to the present invention, a heat conversion element having a pair of membrane electrodes formed on a heat conversion base material is immersed in an electrolytic solution, and one of the membrane electrodes is electrolyzed. Formation of a platinum black film consisting of electrolytically depositing a platinum black film by applying a voltage, characterized in that during electrolysis, a reverse voltage of the electrolytic voltage is applied to the other membrane electrode where electrolytic deposition is not intended. A method is provided.
上記熱変換母材としては、熱トランスデユーサとなりつ
る種々のものが挙げられ、例えば焦電体、サーミスタ母
体、サーモパイル等が適しており、これらのうち焦電体
が好ましい。この焦電体としては前述した公知の種々の
ものが使用可能であり、これらのうち潮解性のないＬ！
ＴａＯ３、Ｐｂ Ｔｉ Ｏ３、ＰＺＴなどが好ましい。As the heat conversion base material, there are various materials that can serve as a heat transducer, such as a pyroelectric body, a thermistor base body, a thermopile, etc., and among these, a pyroelectric body is preferable. As this pyroelectric material, various known materials mentioned above can be used, and among these, L! which is not deliquescent!
TaO3, PbTiO3, PZT, etc. are preferred.
上記膜状電極としては、ＰｔやＡＵ等の蒸着膜やスパッ
タリング膜が適しているが、これら以外の導電性膜が使
用可能でありこの例としては、ＣｒやＮｉ−Ｃｒ蒸看膜
が挙げられる。これらの電極膜厚は０．１〜？、０７ａ
程度が適している。As the above-mentioned film electrode, a deposited film or a sputtered film of Pt, AU, etc. is suitable, but conductive films other than these can also be used, examples of which include Cr and Ni-Cr vaporized films. . The thickness of these electrodes is 0.1~? , 07a
The degree is appropriate.
この発明における電解液としては、白金黒を電解形成し
うる電解質であればよ（、塩化白金酸等の白金酸根を含
有する水溶液が用いられる。これらの電解液中には、電
解用の各種添加剤が含有されていてもよく、その−例と
しては、酢酸鉛等の黒化促進剤が挙げられる。The electrolyte in this invention may be any electrolyte that can electrolytically form platinum black (an aqueous solution containing a platinum acid group such as chloroplatinic acid is used).These electrolytes may contain various additives for electrolysis. Agents may be included, examples of which include blackening accelerators such as lead acetate.
この発明において、白金黒膜の被着形成を意図する一方
の膜状電極は負極側に設定され、所定の電解電圧が印加
される。この際の至適電解電圧は、電極面積、電極間隔
、白金酸濃度、温度等に左右されるが、白金対極を用い
た場合通常、膜状電極の電位が約−０，２〜−０，７Ｖ
（ｖｓ ＡＱ ／ＡｇＣρ）に維持されるように設
定して定電位電解で行なうのが適している。一方、被着
形成を意図しない膜状電極に印加する逆電圧も上記と同
様に条件により異なるが、通常、その電位が約＋１．０
〜−０．２Ｖ （ＶＳ Ａ（ＩＩ ／ＡＯＣΩ）に維
持されるように設定するのが適している。また、白金黒
の被着膜厚は５〜２０−程度が適しており、電解時間を
調整（通常、２０〜６０秒程度）することにより容易に
制御可能である。In this invention, one of the membrane electrodes intended to form a platinum black film is set on the negative electrode side, and a predetermined electrolytic voltage is applied thereto. The optimal electrolytic voltage at this time depends on the electrode area, electrode spacing, platinic acid concentration, temperature, etc., but when a platinum counter electrode is used, the potential of the membrane electrode is usually about -0.2 to -0. 7V
(vs AQ /AgCρ) is preferably maintained at constant potential electrolysis. On the other hand, the reverse voltage applied to the membrane electrode that is not intended to form an adhesion varies depending on the conditions as described above, but usually the potential is about +1.0
It is suitable to set it so that it is maintained at ~-0.2V (VS A (II / AOCΩ). Also, it is suitable that the thickness of the platinum black coating is about 5 to 20V, and the electrolysis time is It can be easily controlled by adjusting (usually about 20 to 60 seconds).
このようにして電解を行なうことにより、一対の膜状Ｎ
極のうちの一方のみに白金黒膜が被着形成される。そし
て、この白金黒膜は、２〜７膚程度の白金粒塊が積重な
った構造の均一な膜であり、とくに赤外線波長が２．５
〜２５４において照度が略１に近い黒化膜である。By performing electrolysis in this way, a pair of membrane-like N
A black platinum film is deposited on only one of the poles. This platinum black film is a uniform film with a structure in which 2 to 7 platinum grains are stacked, and in particular, the infrared wavelength is 2.5.
It is a blackened film with an illuminance close to 1 at ~254.
（ホ）作 用
白金黒の形成を意図しない裏側電極に電解電圧と逆の電
圧が印加されているため、この電極上への白金黒の形成
が防止されることとなる。(E) Effect Since a voltage opposite to the electrolytic voltage is applied to the back side electrode where the formation of platinum black is not intended, the formation of platinum black on this electrode is prevented.
（へ）実施例
１ ｉ Ｔ８０３からなる集電体（１，２Ｘ １．ＯＸ
８ＩＩＩｍ）の両面にスパッタリングによって白金膜
（膜状電極）を形成（膜厚的０．４ｐ：面積的１ｍｍ’
）した。そしてその端部に金リード線を接続した後、該
焦電体を１０ｍｇの酢酸鉛を含有する５７．９ ｍＭの
塩化白金酸水溶液（電解液）に浸漬して電解系を構成し
た。この状態を第１図に示した。図中、２は焦電体、３
Ａ、３Ｂは白金膜、６は電解液、７は対極となる白金電
極、８は電位モニタ用の参照電極（Ａｇ／ＡＣＩ Ｃ＋
電極）を各々示し、９は表側となる白金膜３Ａと対極７
との間に電解電圧を印加する電源、１０は裏側となる白
金膜３８１．：電解電圧と逆の電圧を印加する逆電圧電
源を各々示す。(to) Example 1 i Current collector made of T803 (1,2X 1.OX
8IIIm) by sputtering to form a platinum film (membrane electrode) (film thickness: 0.4 p: area: 1 mm').
)did. After connecting a gold lead wire to the end thereof, the pyroelectric body was immersed in a 57.9 mM chloroplatinic acid aqueous solution (electrolyte) containing 10 mg of lead acetate to construct an electrolytic system. This state is shown in FIG. In the figure, 2 is a pyroelectric substance, 3
A and 3B are platinum films, 6 is an electrolytic solution, 7 is a platinum electrode serving as a counter electrode, and 8 is a reference electrode for potential monitoring (Ag/ACI C+
9 shows the platinum film 3A on the front side and the counter electrode 7.
10 is a platinum film 381. which is the back side. : Indicates a reverse voltage power supply that applies a voltage opposite to the electrolytic voltage.
この状態で、白金膜３Ａの電位が一〇、３Ｖとなるよう
にかつ白金膜３Ｂの電位が十〇、ＩＶとなるように電源
９及び逆電圧電源１０を調整して室温下約１分、無撹拌
下で電解を行なうことにより、白金膜３Ａ上に厚さ約１
０／１２１１の白金黒膜が被着形成され、白金ＩＩ！３
Ｂ上には白金黒膜が全く形成されていない第２図に示す
ごとき熱センサ１を得た。In this state, the power source 9 and the reverse voltage power source 10 were adjusted so that the potential of the platinum film 3A was 10.3 V and the potential of the platinum film 3B was 10.4 V, and the voltage was set at room temperature for about 1 minute. By performing electrolysis without stirring, a layer of approximately 1.
A platinum black film of 0/1211 was deposited and platinum II! 3
A thermal sensor 1 as shown in FIG. 2 was obtained in which no platinum black film was formed on B.
なお、図中、４は白金黒膜、５は金リード線を各々示す
。かかる白金黒膜は、約２〜７膚の白金粒塊が積重なっ
た構成からなる均一なものであり、２．５〜２５虜の赤
外光において照度が１に近いものであった。In the figure, 4 indicates a platinum black film, and 5 indicates a gold lead wire. The platinum black film had a uniform structure consisting of approximately 2 to 7 platinum grains stacked on top of each other, and had an illuminance close to 1 in infrared light of 2.5 to 25 cm.
これに対し、白金膜３Ｂに逆電圧を印加しない通常の方
法で電解を行なった際には、白金膜３Ｂ上にも不均一な
白金黒の形成が認められ、白金膜３Ａ上の白金黒膜の均
一性も不充分なものであつた。On the other hand, when electrolysis is performed in a normal manner without applying a reverse voltage to the platinum film 3B, non-uniform formation of platinum black is observed on the platinum film 3B, and the platinum black film on the platinum film 3A is The uniformity was also insufficient.
なお、上記実施例で得られた熱センサと、膜状電極とし
てＣｒ膜を有し白金黒膜を有ざない従来の熱センサとを
比較したところ、従来の熱センサでは吸光率的６４％で
あるのに対し、実流例の熱センサでは約９５％（反射光
スペクトルの平均値ンと熱吸収性の優れたものであった
。In addition, when comparing the thermal sensor obtained in the above example with a conventional thermal sensor that has a Cr film as a film electrode and does not have a platinum black film, it was found that the conventional thermal sensor had an absorbance of 64%. On the other hand, the thermal sensor in the actual flow example had an average value of reflected light spectrum of about 95% and excellent heat absorption.
（ト）発明の効果
この発明の白金黒膜の形成方法によれば、一対の膜状電
極を形成した熱変換母材の一方の膜状電極上にのみ、効
率良く均一な白金黒膜を形成することができる。従って
、白金黒膜被着素子を安定にかつ分留り良く形成するこ
とができ、また、形成される白金黒膜も熱吸収性の著し
く優れたものである。(g) Effects of the Invention According to the method for forming a platinum black film of the present invention, a uniform platinum black film can be efficiently and uniformly formed only on one film-like electrode of a heat conversion base material on which a pair of film-like electrodes are formed. can do. Therefore, a platinum black film-coated element can be formed stably and with good yield, and the formed platinum black film also has extremely excellent heat absorption properties.
第１図は、この発明の形成方法の一工程を示す構成説明
図、第２図はこの発明の形成方法で熱変換素子上に形成
された白金黒膜を示す構成説明図である。
１・・・・・・熱センサ、 ２・・・・・・焦電体、
３Ａ、３Ｂ・・・・・・白金膜、４・・・・・・白金黒
膜、５・・・・・・金リード線、 ６・・・・・・電
解液、７・・・・・・白金電極、 ８・・・・・・
参照電極、９・・・・・・電源、 １０・・・・
・・逆電圧電源。
第 １ 図
第２図FIG. 1 is a structural explanatory diagram showing one step of the forming method of the present invention, and FIG. 2 is a structural explanatory diagram showing a platinum black film formed on a heat conversion element by the forming method of the present invention. 1... Heat sensor, 2... Pyroelectric body,
3A, 3B...Platinum film, 4...Platinum black film, 5...Gold lead wire, 6...Electrolyte, 7...・Platinum electrode, 8...
Reference electrode, 9...Power supply, 10...
...Reverse voltage power supply. Figure 1 Figure 2
Claims (1)
子を電解液中に浸漬しその膜状電極の一方に電解電圧を
印加して白金黒膜を電解被着することからなり、電解中
に電解被着を意図しない他方の膜状電極に電解電圧の逆
電圧を印加することを特徴とする白金黒膜の形成方法。 ２、電解電圧が約−０．２〜−０．７（ｖｓＡｇ／Ａｇ
Ｃｌ）Ｖであり逆電圧が、約＋１．０〜−０．２Ｖ（ｖ
ｓＡｇ／ＡｇＣｌ）である特許請求の範囲第１項記載の
形成方法。[Claims] 1. A heat conversion element having a pair of film electrodes formed on a heat conversion base material is immersed in an electrolytic solution, and an electrolytic voltage is applied to one of the film electrodes to electrolyze the platinum black film. 1. A method for forming a platinum black film, which comprises applying a voltage opposite to the electrolytic voltage to the other membrane electrode not intended for electrolytic deposition during electrolysis. 2. Electrolytic voltage is approximately -0.2 to -0.7 (vsAg/Ag
Cl)V, and the reverse voltage is approximately +1.0 to -0.2V (v
sAg/AgCl).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61312751A JPS63168518A (en) | 1986-12-29 | 1986-12-29 | Method for forming platinum black film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61312751A JPS63168518A (en) | 1986-12-29 | 1986-12-29 | Method for forming platinum black film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63168518A true JPS63168518A (en) | 1988-07-12 |
Family
ID=18032981
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61312751A Pending JPS63168518A (en) | 1986-12-29 | 1986-12-29 | Method for forming platinum black film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63168518A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5248874B1 (en) * | 1971-04-26 | 1977-12-13 |
-
1986
- 1986-12-29 JP JP61312751A patent/JPS63168518A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5248874B1 (en) * | 1971-04-26 | 1977-12-13 |
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